Chlorine-containing compound



' too great an excessun avorably a ects' the phate salt.

Prams Sept. 29, 1925.

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Ilo Drawing.

To. all whom it may concern: Be it known that I, LEWIS D. MATHIAB, a citizen of the United States, residin at Chicago Heights, in the county of k and State of Illinois, have invented a new and useful Improvement in Chlorine-Con- 'taining Compounds, of which the following is a specification. 0

' This invention relates to improvements 1n compounds containing chlorine in an avallable s form primarily intended for use for germicidal and disinfectant purposes.

In accordance with the present Invention, a material containing available chlorine "is produced in a form of a compound, hitherto unknown, having the character of a double salt of normal sodium phosphate and hy ochlorite, the proportion of available chl drine being at least 1% by weight.

In carrying out the process of my invention, I may react upon a solutionof a sodium phosphate salt with a. hypochlor te in the presence of suflicient caustic alkali to insure the presence of the normal phos- Thus, I may use the normal sodium phosphate or an acid sodium phosphate or. even hosphoric acid together with suflicient caust1c alkali (as sodium hydroxide, for'example) to form the normal salt 7 and provide at least a slight excess of alkali. The hypochlorite may be added as such, or may be formed in the reaction mixture by providing a sufficient excess of sodium hydroxide therein and passing chlorine into it. The following examples illustrate variousmethods in which my invention may be carried into effect. p I

1. Trisodium phosphate (Na-$0 .12 H O) is dissolved in sufiicient water to form a saturated solution at the temperature at which the reaction is. carried out, which should be at least 15 C. and should preferably be about 50, O. 2% or higher (prefer. ably from 2 to10%) (on the phosphate)-- of sodium hydroxide'is added to the solution and chlorine is passed'thereinto slowly until from 5 to or. higher (on the hosphate') of available chlorine has been a ded, the temperature being maintained about C.,:and preferably about C. More than 10% of the alkali ma be emplo ed, but

economy and yields of the operation Ex cessive proportions of-chlorine have s milar unfavorable results. The reaction nuxture Application filed June-2a, 192 4. sumac. 121,934.

is then cooled slowly and colorless crystals of the double salt of the phosphate and hypochlorite settle out. The composition of these crystals has not been termined. Their wei ht varies from v to 100% of the weight 0% phos hate originally employed and their availab e chlorine content from 1.25 to 3%. By using saturated solutions of sodium phosphate containing 10 to 20% of sodium hydroxide and passing chlorine through the solution until a test of the liquor showed the presence of free chlorine, on subsequent crystallization cr stals containing from 2.5 to 4% of availa le chlorine were obtained.

2. On mixing concentrated solutions of an acid sodium phosphate, .such as the disoc nrcaeonn renrs, ILLINo'Is, Assrenon 'ro VICTOR onmlcn. wonxs, A coaromnon or ILLINOIS.

precisely dei dium phosphate, sodium hydroxide and sodium hypochlorite at temperatures above .15 0., crystals of the double salt are likewise obtained. Thus, by mlxing a saturated solution of crystalline disodium phosphate with a solution of sodium hydroxide suflicient to provide 10 to 12% of sodium hydroxide on the disodium phosphate, and suflicient saturated solution of sodium by 0- chlorite to provide 5 to 10% of availa le chlorine by weight based on weight of disodium phosphate and crystallizing the resulting mixture, crystals of the double salt were obtained, containing from 2 to 4% of availablechlorine. Less concentrated solutions may be employed, if desired; for example, the .disoda liquor obtained in the manufacture of disodium phosphate may be employedz I In the various methods of operating in ac-' cordance with this invention, a considerable proportion of the available sodium phosphate remains in the mother liquor, from two-thirds to three-fourths being precipitated in theform of the doublesalt. The mother liquor also contains a considerableproportion (from- 4,0 to-60%) of the chlorine used in carrying out the reaction. 'It has been found that this mother liquor may be made use of by adding thereto sufiicient sodium phosphate or acid sodium phosphate v(as disodium phos hate), alkali (for example, sodium hy roxide) and chlorine, either as chlorine or sodium hypochlorite to restore the conditions originally \prevailing in the solut1on before precipitation or crystallization of the double salt, the temperature beingbrought to above 15 0., say

' mately 26 at C. before adding the hypo-- phosphate,

about 50 (1., while this is being done.

cooling 8'. further crystallization takes place.

In each crystalline substance, readily soluble an containing 1% or more available chlorine.

' The mother liquor remaining after removal of the crystals may also be employed in diluting the reaction mixture when the reaction is carried out with more dilute solutions. as in the. following example:

3. Disoda liquor, containing dis0d1um phosphate having a Baum gravity of 32 to 40 is used. Caustic soda solution (40 Baum) is added in quantities sufiicient to make up the calculated amount necessar for forming :the trisodium phosphate an providing a slight excess, and sodlumhypochlorite solution (say 33 Baum) is then added in amount su cient to give approximately two to two and one-half times the percentage of chlorine desired in the double salt product. Thus, if a product contaming 3% available chlorine is desired, the hypochlorite supplied should be calculated on the basis of. 6 t0 7%% available chlorine on the weight of or stalline disodium phosphate in solution. from a preceding finished batch (as herein;

' after set forth is then added to bring the solution to a aum gravity of approxichlorite to the solution. The mixture is allowed to cool to, say, 20 to 23 C. slowly and the crystalline double salt separated out is removed. The mother liquor, which. has a Baum gravity of 13 to 14 may separately worked up, the proper proportions of alkali and chlorine being supplied therein, or ma be used to dilute the next batch of disc iumphosplhate liquor and alkali treated before the ypochlorite solution is added thereto.

' I claim:

1. A compound of a normal phosphate and "a hypochlorite ofsodium, having at least 1% of available ch orine.

. 2. A compound of a, normal phosphate and a hypochlorite ofsodium having 3% of available chlorine.

3- The method of forming a compound containing available chlorine comprisin providing in an aqueous solution norina sodium phosphate and an alkali metal hypochlorite, the temperature being in excess of 15 0., and separating the resulting compound by crystallization.

4. The method of providing a compound containing available chlorine comprising the steps of adding to a concentrated solution of case the double salt is a colorless ater or mother liquor alkali metal hypochlorlte and separating the resulting-com und. v

5. The met 0d of forming a compound On a normal sodiumlpho's hate a solution of an containing available chlorine comprising adding soluble alkali to a concentrated solution of a normal sodium phosphate at a temperature above 15, 0., and passing chlorine through the solution,

6. The method of forming a compound containing available chlorine which comprises maintaining a saturated solution of normal sodium phosphate at 50 C., providing sodium hypochlorite in the solution, and cooling the liquor to crystallize out the desired compound. V

7. The method of forming a compound containing available chlorine comprisin introducing into a solution ofnormal so um phosphate a solution. of an alkali metal hypochlorite. v

8. The method of forming a compound containing available chlorine which comprises adding to a' solution of disodium phosphate suflicient soluble alkali to form the normal phosphate, and adding to the resulting solution a concentrated solution of sodium hypochlorite.

9. The method of forming a material combining sodium phosphate and sodium hypochlorite which comprises adding to a solution of disodium phosphate suificient sodium hydroxide solution to form the normal phosphate, and adding a sodium hypochlorite solution to the resulting solution. a

10. The method of forming a material combining sodium phosphate and sodium hypochlorite which comprises adding to aconcentrated disodium phosphate solution sufiicient sodium hydroxide solution to form the trisodium phosphate, diluting the solution to- 26 Baum while maintalning it at 50 C. and addingthereto an alkali metal hypochlorite solution. r

11- The method of forming a materia combining sodium phosphate and sodium hypochlorite which comprises adding to a concentrated disodium. osphat'e solution suflicient sodium hydroxi e solution to 'form the trisodium phosphate, diluting the solution to 26 Baum while maintaming it at 50 C. and adding thereto an alkali metal hypochlorite' solution, cooling the resulting solution, thereby crystallizing out the compound, and employing'the mother liquor to dilute a succeeding batch undergoing treatment.

LEWIS 1). MATHIAS. 

